CN110042652A - A kind of expandable flame retardant coating solution and its application - Google Patents
A kind of expandable flame retardant coating solution and its application Download PDFInfo
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Abstract
Description
技术领域technical field
本发明涉及一种织物用阻燃剂，特别是涉及一种用于涂覆在织物上起阻燃作用的环境友好型膨胀阻燃涂层液。The invention relates to a flame retardant for fabrics, in particular to an environment-friendly intumescent flame retardant coating liquid used for coating on fabrics to play a flame retardant role.
背景技术Background technique
2018年1～8月，全国共有16.61万起火灾，致933人死亡，560人受伤，直接财产损失20.53亿元。火灾的危害性推动了阻燃材料的发展。但阻燃材料在满足国家安全标准的同时，也要符合高效、环保和绿色等发展理念，避免造成二次危害。From January to August 2018, there were 166,100 fires nationwide, resulting in 933 deaths, 560 injuries, and direct property losses of 2.053 billion yuan. The hazard of fire has promoted the development of flame retardant materials. However, while meeting national safety standards, flame retardant materials must also comply with development concepts such as high efficiency, environmental protection and greenness to avoid secondary hazards.
纺织品与人类的生活息息相关，已经渗透到国民经济的各个领域，如建筑、土地、工业、医药、汽车、生态、防护和运动等。纺织品阻燃一直是阻燃研究领域的重中之重。其中，涤纶位于合成纤维之首，具有一系列优良的性能，如强度高、耐热、耐光、耐磨、耐腐蚀、弹性好、热塑性好、化学性能稳定等，广泛应用于服装外套、沙发、窗帘装饰、以及国防、工业用布等领域。Textiles are closely related to human life and have penetrated into various fields of the national economy, such as construction, land, industry, medicine, automobiles, ecology, protection and sports. The flame retardancy of textiles has always been the top priority in the field of flame retardant research. Among them, polyester ranks first in synthetic fibers and has a series of excellent properties, such as high strength, heat resistance, light resistance, wear resistance, corrosion resistance, good elasticity, good thermoplasticity, stable chemical properties, etc. It is widely used in clothing jackets, sofas, Curtain decoration, as well as national defense, industrial cloth and other fields.
涤纶织物极易燃烧，其在受热分解时会产生大量的烟雾颗粒和可燃性物质，并产生大量的热量和烟气，给人们的生活和生命带来不可估量的损失。因此，阻燃涤纶织物的研究意义重大。Polyester fabric is extremely flammable, and when it is thermally decomposed, it will produce a large number of smoke particles and combustible substances, and generate a large amount of heat and smoke, which will bring immeasurable losses to people's lives and lives. Therefore, the research on flame retardant polyester fabrics is of great significance.
目前应用于涤纶的阻燃剂主要包括卤系阻燃剂和非卤系阻燃剂两大类。其中，卤系阻燃剂在实际应用中会产生许多问题，例如腐蚀设备、燃烧释放有毒产物等，因此已逐渐退出阻燃剂的队伍。非卤系阻燃剂主要包括磷系、无机型和膨胀型阻燃剂。其中磷系阻燃剂在燃烧过程中会产生有毒中间体，而无机型阻燃剂的添加量较大。The flame retardants currently used in polyester mainly include halogenated flame retardants and non-halogenated flame retardants. Among them, halogen-based flame retardants will cause many problems in practical application, such as corrosion of equipment, release of toxic products when burning, etc., so they have gradually withdrawn from the ranks of flame retardants. Non-halogen flame retardants mainly include phosphorus-based, inorganic and intumescent flame retardants. Among them, phosphorus-based flame retardants will produce toxic intermediates during the combustion process, while inorganic flame retardants are added in larger amounts.
膨胀型阻燃剂(IFR)属于环境友好型阻燃体系，主要包含磷、氮两种阻燃元素，通常包括酸源、炭源和气源。其中酸源主要发挥脱水效应，作为脱水剂；炭源一般为富含碳原子的多羟基化合物；气源一般为受热可释放挥发产物的化合物。IFR体系不仅具有无卤、环保、低烟、低毒、低添加量的阻燃特性，还实现了低添加量下的高效阻燃，成为近年来国内外阻燃领域研究的热点，被广泛应用于高分子聚合物中。但在涤纶织物上的应用鲜有报道。Intumescent flame retardant (IFR) is an environment-friendly flame retardant system, mainly containing phosphorus and nitrogen two flame retardant elements, usually including acid source, carbon source and gas source. Among them, the acid source mainly exerts the dehydration effect as a dehydrating agent; the carbon source is generally a polyhydroxy compound rich in carbon atoms; the gas source is generally a compound that can release volatile products when heated. The IFR system not only has the flame retardant properties of halogen-free, environmental protection, low smoke, low toxicity and low dosage, but also achieves high efficiency flame retardant at low dosage. in high molecular weight polymers. However, the application on polyester fabrics is rarely reported.
膨胀阻燃剂分为多组分和单组分阻燃剂。其中多组分阻燃剂是由两种或多种阻燃剂通过复配技术构建膨胀阻燃体系，由于阻燃剂种类多，需要考虑多重界面的相容性问题。单组份阻燃剂是“三源一体”化，通过物理或化学方式(如微胶囊技术)将多组分阻燃剂构建为一体化阻燃剂，不仅可以改善阻燃剂与基体的相容性，还能极大的改善其分散性。单组份阻燃剂已经成为目前研究的重点方向。Intumescent flame retardants are divided into multi-component and single-component flame retardants. Among them, the multi-component flame retardant is an intumescent flame retardant system constructed by two or more flame retardants through compounding technology. Due to the variety of flame retardants, the compatibility of multiple interfaces needs to be considered. One-component flame retardants are "three-in-one", and multi-component flame retardants are constructed into integrated flame retardants by physical or chemical means (such as microcapsule technology), which can not only improve the phase between the flame retardant and the matrix. It can also greatly improve its dispersibility. One-component flame retardants have become the focus of current research.
何敏等(PP/LGF复合材料的膨胀性阻燃与协效阻燃性能[J]. 工程塑料应用,2017(6): 29-34.)采用膨胀型阻燃剂及协效剂海泡石(SP)对长玻璃纤维增强聚丙烯(PP/LGF)复合材料进行阻燃。结果表明，含有1% SP、21% IFR的PP/LGF/IFR/SP阻燃复合材料的LOI值为29.6%，垂直燃烧等级达到V-0级，可以有效降低复合材料的热释放速率峰值，且燃烧时产生致密的炭层覆盖于玻璃纤维表面。He Min et al. (Intumescent flame retardant and synergistic flame retardant properties of PP/LGF composites [J]. Application of Engineering Plastics, 2017(6): 29-34.) Using intumescent flame retardant and synergist seafoam Fire retardation of long glass fiber reinforced polypropylene (PP/LGF) composites with stone (SP). The results show that the LOI value of the PP/LGF/IFR/SP flame retardant composite containing 1% SP and 21% IFR is 29.6%, and the vertical combustion grade reaches V-0, which can effectively reduce the peak heat release rate of the composite material. And when burning, a dense carbon layer covers the surface of the glass fiber.
杨尚军等(GP/APP膨胀阻燃体系对硅橡胶复合材料阻燃及抑烟性能的影响[J].中国安全生产科学技术, 2018, 14(11): 146-150.)探究了石墨粉(GP)与聚磷酸铵(APP)膨胀阻燃体系对硅橡胶复合材料的阻燃及抑烟特性的影响。研究结果表明，与单独添加膨胀阻燃剂APP的阻燃硅橡胶相比，添加GP/APP膨胀阻燃体系可以有效提升燃烧过程中形成膨胀炭层的致密度。Yang Shangjun et al. (The effect of GP/APP intumescent flame retardant system on the flame retardant and smoke suppression properties of silicone rubber composites [J]. China Safety Production Science and Technology, 2018, 14(11): 146-150.) explored the graphite powder ( Effects of GP) and ammonium polyphosphate (APP) intumescent flame retardant systems on the flame retardant and smoke suppression properties of silicone rubber composites. The research results show that the addition of GP/APP intumescent flame retardant system can effectively improve the density of the intumescent carbon layer formed during the combustion process, compared with the flame retardant silicone rubber added with the intumescent flame retardant APP alone.
Zhou Yi等(Reach on P/N Type Intumescent Flame Retardant for PolyesterFabric[J]. Advanced Materials Research, 2013, 785-786: 714-717.)将含磷阻燃剂与APP溶于水中，制备出膨胀阻燃液，并通过二浸二轧方式对涤纶织物进行了阻燃整理。研究发现，该阻燃剂能有效改善涤纶织物在燃烧过程中的熔滴现象，并有效降低织物的热释放，但并未介绍阻燃剂的耐水解性能。Zhou Yi et al. (Reach on P/N Type Intumescent Flame Retardant for PolyesterFabric[J]. Advanced Materials Research, 2013, 785-786: 714-717.) dissolved phosphorus flame retardant and APP in water to prepare expansion resistance The flame retardant finishing of the polyester fabric was carried out by two dipping and two rolling methods. The study found that the flame retardant can effectively improve the droplet phenomenon of polyester fabrics during the combustion process and effectively reduce the heat release of the fabrics, but the hydrolysis resistance of the flame retardants was not introduced.
碳微球(CMSs)是一种由多层石墨片环绕构成的，具有类富勒烯笼状结构的新兴球型碳材料，其具有良好的阻燃性能，可以用来作为膨胀阻燃体系的新型炭源。CMSs受热燃烧后可以在聚合物基体表面形成炭层，阻止基体表面氧气和热量的进入，这种阻燃方式被称为凝聚相阻燃。CMSs在低添加量下就可以显著提高聚合物的LOI值，且这一结论已被前期工作验证。但是，CMSs极易发生团聚，而且不能有效降低聚合物产生的烟气，限制了其在很多应用领域的应用(如军服和防护服等)。Carbon microspheres (CMSs) are an emerging spherical carbon material with a fullerene-like cage structure surrounded by multi-layer graphite sheets. New carbon source. After CMSs are heated and burned, a carbon layer can be formed on the surface of the polymer matrix to prevent the entry of oxygen and heat on the surface of the matrix. This flame retardant method is called condensed phase flame retardant. CMSs can significantly improve the LOI value of polymers at low addition levels, and this conclusion has been verified by previous work. However, CMSs are prone to agglomeration and cannot effectively reduce the smoke generated by polymers, which limits their application in many application fields (such as military uniforms and protective clothing, etc.).
聚磷酸铵(APP)作为一种无机型磷系阻燃剂，具有含磷量大、含氮量高，以及热稳定性好、分散性好、毒性低等优点。APP可以作为膨胀阻燃体系中的酸源和气源，促使聚合物分解时的脱水和碳化，并能释放不燃性气体发挥稀释氧气的作用，从而提高聚合物的成炭率。但当APP单独作用时，并不能提高聚合物的阻燃性，相反还极大的降低了聚合物的力学性能。Ammonium polyphosphate (APP), as an inorganic phosphorus-based flame retardant, has the advantages of large phosphorus content, high nitrogen content, good thermal stability, good dispersibility, and low toxicity. APP can be used as the acid source and gas source in the intumescent flame retardant system to promote the dehydration and carbonization of the polymer during decomposition, and can release incombustible gas to dilute oxygen, thereby improving the carbonization rate of the polymer. However, when APP acts alone, it cannot improve the flame retardancy of the polymer, on the contrary, it also greatly reduces the mechanical properties of the polymer.
CN 109181248A公开了一种聚磷酸铵包覆碳微球阻燃剂的制备方法，其以CMSs为炭源，APP为酸源和气源，将CMSs硅烷化改性后，与APP悬浊液混合进行回流反应，以APP包覆硅烷化改性CMSs制备得到CMSs-APP阻燃剂，并将该阻燃剂以共混的方式添加在PET材料中制备出阻燃PET复合材料，提高了PET材料的阻燃性能。CN 109181248A discloses a preparation method of ammonium polyphosphate coated carbon microsphere flame retardant, which uses CMSs as carbon source, APP as acid source and gas source, silanized and modified CMSs, and mixed with APP suspension The CMSs-APP flame retardant is prepared by coating the silanized modified CMSs with APP, and the flame retardant is added to the PET material in a blending manner to prepare a flame retardant PET composite material, which improves the performance of the PET material. flame retardant properties.
然而，在阻燃剂与PET材料的熔融共混过程中可能会产生一些来源于阻燃剂的小分子物质，以存在有这些小分子物质的PET材料进行纺丝，所获得纤维的各项物理性能可能会受到一定的影响。However, some small molecular substances derived from flame retardants may be produced during the melt blending process of flame retardants and PET materials. Spinning with PET materials with these small molecular substances present will result in the physical properties of the fibers obtained. Performance may be affected to some extent.
后整理法是对织物进行阻燃处理的另一种常用方法，其采用浸渍烘焙、喷涂等方式对织物成品进行表面处理，具有操作简单、成本低廉、适用性广等优势，且由于阻燃剂是直接覆盖在织物表面，不仅不会改变织物的各项物理性能，而且阻燃效果更加高效。但后整理法也存在着一些较难解决的问题，例如阻燃剂在涤纶织物上的附着性较差，且耐水洗性较差。The post-finishing method is another common method for flame retardant treatment of fabrics. It uses dipping, baking, spraying, etc. to treat the surface of the finished fabric. It has the advantages of simple operation, low cost, and wide applicability. It is directly covered on the surface of the fabric, which not only does not change the physical properties of the fabric, but also has a more efficient flame retardant effect. However, the post-finishing method also has some difficult problems to solve, such as poor adhesion of flame retardants on polyester fabrics and poor washing resistance.
发明内容SUMMARY OF THE INVENTION
本发明的目的是提供一种具有良好粘附性能的膨胀阻燃涂层液，以其采用后整理方式对涤纶织物进行阻燃整理，可以极大的提高涤纶织物的阻燃性能，并显著提高织物的耐水洗性。The purpose of the present invention is to provide an intumescent flame retardant coating liquid with good adhesion properties, which can greatly improve the flame retardant properties of polyester fabrics and significantly improve the flame retardant finishing of polyester fabrics by using post-finishing methods. Washability of the fabric.
本发明所述的膨胀阻燃涂层液是以CMSs-APP为阻燃剂，将其分散在混合粘合剂溶液中得到的阻燃涂层液，其中，所述的阻燃剂CMSs-APP是CN 109181248A中制备的阻燃剂，所述的混合粘合剂溶液是以DOPO与PVFA组成混合粘合剂，溶解在其的可溶性溶剂中得到的溶液。The intumescent flame retardant coating liquid of the present invention is a flame retardant coating liquid obtained by dispersing CMSs-APP as a flame retardant in a mixed binder solution, wherein the flame retardant CMSs-APP It is a flame retardant prepared in CN 109181248A. The mixed adhesive solution is a solution obtained by dissolving DOPO and PVFA to form a mixed adhesive in its soluble solvent.
本发明所述的混合粘合剂中，DOPO是化合物9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物的英文缩写，其在常温下会产生脆性膜，容易在受力时断裂。PVFA化学名称聚乙烯醇缩甲乙醛，兼具聚乙烯醇缩甲醛和聚乙烯醇缩乙醛的优良性能，容易形成柔软、但强度较低的膜。本发明利用两者复合成膜，获得了一种高质量且具有韧性的成膜物质，且基于DOPO较好的耐水性、耐氧化性和较高的热稳定性，能够获得耐水性、耐老化性能优异的涂层结构。In the mixed adhesive of the present invention, DOPO is the English abbreviation of the compound 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, which produces a brittle film at room temperature, which is easy to Broken under stress. The chemical name of PVFA is polyvinyl methyl acetal, which has both the excellent properties of polyvinyl formal and polyvinyl acetal, and is easy to form a soft, but low-strength film. The present invention utilizes the two composite films to obtain a high-quality and tough film-forming material, and based on the better water resistance, oxidation resistance and high thermal stability of DOPO, water resistance, aging resistance can be obtained. Excellent performance coating structure.
进一步地，本发明所述的混合粘合剂中，DOPO与PVFA的质量比为1∶1～4。Further, in the mixed adhesive of the present invention, the mass ratio of DOPO to PVFA is 1:1-4.
更进一步地，本发明所述的阻燃涂层液中，所述阻燃剂CMSs-APP与混合粘合剂的用量质量比为1∶2～10。Further, in the flame retardant coating liquid of the present invention, the amount and mass ratio of the flame retardant CMSs-APP to the mixed adhesive is 1:2-10.
进而，本发明所制备的阻燃涂层液中，所述阻燃剂CMSs-APP的质量浓度优选为5～50g/L。Furthermore, in the flame retardant coating liquid prepared by the present invention, the mass concentration of the flame retardant CMSs-APP is preferably 5-50 g/L.
本发明中，所述混合粘合剂的可溶性溶剂是任何一种可以同时溶解DOPO和PVFA的有机溶剂，例如，可以是烷烃类溶剂、芳香烃类溶剂、卤代烃类溶剂、醇类溶剂、醚类溶剂等。基于大部分有机溶剂都有一定的毒性，从环境友好的角度考虑，本发明优选采用无毒的无水乙醇作为所述混合粘合剂的溶剂。In the present invention, the soluble solvent of the mixed adhesive is any organic solvent that can dissolve DOPO and PVFA at the same time, such as alkane solvents, aromatic hydrocarbon solvents, halogenated hydrocarbon solvents, alcohol solvents, ether solvents, etc. Since most organic solvents have certain toxicity, from the viewpoint of environmental friendliness, the present invention preferably adopts non-toxic anhydrous ethanol as the solvent of the mixed adhesive.
本发明进而提供了一种所述膨胀阻燃涂层液的制备方法，所述制备方法具体包括下述步骤。The present invention further provides a preparation method of the intumescent flame retardant coating liquid, and the preparation method specifically includes the following steps.
1)、将阻燃剂CMSs-APP分散在无水乙醇中得到阻燃剂的乙醇分散液。1) Disperse the flame retardant CMSs-APP in absolute ethanol to obtain an ethanol dispersion of the flame retardant.
2)、将DOPO与PVFA以质量比1∶1～4混合后，以无水乙醇溶解得到混合粘合剂溶液。2), after mixing DOPO and PVFA in a mass ratio of 1:1-4, and dissolving in absolute ethanol to obtain a mixed binder solution.
3)、按照阻燃剂与混合粘合剂的质量比为1∶2～10，将所述阻燃剂的乙醇分散液加入所述混合粘合剂溶液中，80～85℃下反应20～40min，制备得到所述膨胀阻燃涂层液。3), according to the mass ratio of the flame retardant and the mixed adhesive to be 1:2～10, add the ethanol dispersion of the flame retardant to the mixed adhesive solution, and react at 80～85 ℃ for 20～ 40 min to prepare the intumescent flame retardant coating liquid.
其中，本发明优选将阻燃剂CMSs-APP加入到无水乙醇中，采用超声处理的手段得到所述阻燃剂的乙醇分散液。Among them, in the present invention, the flame retardant CMSs-APP is preferably added into absolute ethanol, and the ethanol dispersion of the flame retardant is obtained by means of ultrasonic treatment.
进一步地，本发明将所述阻燃剂CMSs-APP预先在80～100℃下干燥12～24h后再使用。Further, in the present invention, the flame retardant CMSs-APP is pre-dried at 80-100° C. for 12-24 hours before use.
本发明制备的膨胀阻燃涂层液可以作为阻燃剂，用于涤纶织物的阻燃整理处理中。The intumescent flame retardant coating liquid prepared by the invention can be used as a flame retardant in the flame retardant finishing treatment of polyester fabrics.
具体地，是以本发明制备的膨胀阻燃涂层液作为整理剂，涂覆在涤纶织物表面，以制备阻燃涤纶织物。Specifically, the intumescent flame-retardant coating liquid prepared by the present invention is used as a finishing agent to coat the surface of the polyester fabric to prepare the flame-retardant polyester fabric.
更具体地，是将待整理的涤纶织物浸渍到上述阻燃涂层液中，采用溶液浸渍法，将阻燃涂层液涂覆到涤纶织物表面，干燥后，制备得到具有良好阻燃性能的阻燃涤纶织物。More specifically, the polyester fabric to be finished is dipped into the above-mentioned flame retardant coating liquid, and the flame retardant coating liquid is coated on the surface of the polyester fabric by the solution dipping method, and after drying, the flame retardant coating liquid with good flame retardant performance is prepared. Flame retardant polyester fabric.
本发明进而提供了所述阻燃涤纶织物的制备方法，具体包括下述步骤。The present invention further provides a method for preparing the flame retardant polyester fabric, which specifically includes the following steps.
1)、对涤纶织物进行碱处理，以增加涤纶织物表面粗糙度，以利于阻燃涂层液的粘合。1) Alkali treatment of polyester fabrics to increase the surface roughness of polyester fabrics to facilitate the adhesion of the flame retardant coating liquid.
2)、将碱处理后的涤纶织物浸渍在阻燃涂层液中并匀速提拉1～10min，以均匀涂覆阻燃涂层液。2) Dip the alkali-treated polyester fabric in the flame retardant coating solution and pull it at a constant speed for 1-10 minutes to uniformly coat the flame retardant coating solution.
3)、涂覆阻燃涂层液的涤纶织物干燥后，得到阻燃涤纶织物。3), after the polyester fabric coated with the flame retardant coating liquid is dried, the flame retardant polyester fabric is obtained.
进而，本发明所述的碱处理是将涤纶织物浸泡于浓度1～5g/L的氢氧化钠水溶液中20～60min，并在70～100℃下干燥5～10h。Furthermore, in the alkali treatment of the present invention, the polyester fabric is soaked in an aqueous sodium hydroxide solution with a concentration of 1-5 g/L for 20-60 minutes, and dried at 70-100° C. for 5-10 hours.
进一步地，本发明所述浸渍过程应不少于2次，最后在70～100℃下干燥2～5h，得到阻燃涤纶织物。Further, the impregnation process of the present invention should be no less than 2 times, and finally the flame retardant polyester fabric is obtained by drying at 70-100° C. for 2-5 hours.
本发明通过比较简单的方法制备出膨胀阻燃涂层液，并采用溶液浸渍法制备出CA涂层涤纶织物。获得了综合性能优异的阻燃涤纶织物。The invention prepares the intumescent flame retardant coating solution by a relatively simple method, and adopts the solution dipping method to prepare the CA coated polyester fabric. A flame retardant polyester fabric with excellent comprehensive properties was obtained.
本发明通过比较简单的方法制备出膨胀阻燃涂层液，并采用溶液浸渍法对涤纶织物进行后整理处理，获得了综合性能优异的阻燃涤纶织物，不仅LOI值可以达到28%以上，并通过垂直燃烧的B1级，而且织物的经向和纬向拉伸强度分别提高了11.5%和42.9%，经过10次水洗后，织物的LOI值仍能达到27%以上，满足阻燃性能需求。The invention prepares an intumescent flame retardant coating solution by a relatively simple method, and adopts a solution dipping method to perform post-finishing treatment on the polyester fabric, so as to obtain a flame retardant polyester fabric with excellent comprehensive properties. Not only the LOI value can reach more than 28%, but also Through the B1 grade of vertical burning, and the tensile strength of the fabric in the warp direction and weft direction is increased by 11.5% and 42.9% respectively, after 10 times of washing, the LOI value of the fabric can still reach more than 27%, which meets the requirements of flame retardant performance.
附图说明Description of drawings
图1是不同处理涤纶织物的扫描电镜图。Figure 1 is a scanning electron microscope image of polyester fabrics with different treatments.
图2是不同处理涤纶织物的释热速率与总热释放曲线。Figure 2 is the heat release rate and total heat release curves of different treated polyester fabrics.
图3是不同处理涤纶织物的拉伸强度对比图。Figure 3 is a comparison chart of tensile strength of polyester fabrics with different treatments.
图4是熔融共混制备CA/PET复合材料的拉伸强度对比图。Figure 4 is a comparison chart of tensile strength of CA/PET composites prepared by melt blending.
具体实施方式Detailed ways
以下结合附图对本发明的具体实施例做进一步的说明。The specific embodiments of the present invention will be further described below with reference to the accompanying drawings.
下述实施例仅为本发明的优选技术方案，并不用于对本发明进行任何限制。对于本领域技术人员而言，本发明可以有各种更改和变化。凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。The following embodiments are only preferred technical solutions of the present invention, and are not intended to limit the present invention. Various modifications and variations of the present invention are possible for those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included within the protection scope of the present invention.
以下实施例中使用的CMSs-APP阻燃剂为按照CN 109181248A中公开方法制备得到的阻燃剂。The CMSs-APP flame retardant used in the following examples is a flame retardant prepared according to the method disclosed in CN 109181248A.
实施例1。Example 1.
取2g CMSs-APP阻燃剂，加入到20mL无水乙醇中，30℃下超声处理30min，得到CMSs-APP阻燃剂分散液。Take 2 g of CMSs-APP flame retardant, add it to 20 mL of absolute ethanol, and ultrasonically treat it for 30 min at 30 °C to obtain a CMSs-APP flame retardant dispersion.
向加有50mL无水乙醇的三颈烧瓶中缓慢加入1g DOPO、1g PVFA，室温下搅拌20min后，再将上述CMSs-APP阻燃剂分散液全部倒入三颈烧瓶中，加热至80℃反应30min，制备得到CA阻燃涂层液。Slowly add 1 g DOPO and 1 g PVFA to a three-necked flask with 50 mL of anhydrous ethanol, stir at room temperature for 20 min, then pour all the above-mentioned CMSs-APP flame retardant dispersion into the three-necked flask, and heat to 80 °C for reaction After 30 min, the CA flame retardant coating solution was prepared.
将涤纶织物浸渍于2g/L的NaOH溶液中碱处理30min后，取出，80℃下干燥8h。The polyester fabric was immersed in a 2g/L NaOH solution for 30min alkali treatment, then taken out and dried at 80°C for 8h.
再把碱处理后的涤纶织物浸渍在上述CA阻燃涂层液中，匀速提拉2min，以均匀涂覆上CA阻燃涂层液。Then, the alkali-treated polyester fabric was dipped in the above-mentioned CA flame retardant coating solution, and pulled at a constant speed for 2 min to evenly coat the CA flame retardant coating solution.
取出涂覆后的涤纶织物，70℃下干燥5h，制备得到CA涂层阻燃涤纶织物CAP1。The coated polyester fabric was taken out and dried at 70 °C for 5 h to prepare the CA-coated flame retardant polyester fabric CAP1.
实施例2。Example 2.
取2g CMSs-APP阻燃剂，加入到30mL无水乙醇中，40℃下超声处理40min，得到CMSs-APP阻燃剂分散液。Take 2 g of CMSs-APP flame retardant, add it to 30 mL of absolute ethanol, and ultrasonically treat it at 40°C for 40 min to obtain a CMSs-APP flame retardant dispersion.
向加有80mL无水乙醇的三颈烧瓶中缓慢加入1g DOPO、3g PVFA，室温下搅拌40min后，再将上述CMSs-APP阻燃剂分散液全部倒入三颈烧瓶中，加热至85℃反应30min，制备得到CA阻燃涂层液。Slowly add 1 g DOPO and 3 g PVFA to a three-necked flask with 80 mL of absolute ethanol, stir at room temperature for 40 min, then pour all the above-mentioned CMSs-APP flame retardant dispersion into the three-necked flask, and heat to 85 °C for reaction After 30 min, the CA flame retardant coating solution was prepared.
将涤纶织物浸渍于2g/L的NaOH溶液中碱处理60min后，取出，90℃下干燥7h。The polyester fabric was immersed in a 2g/L NaOH solution for 60min alkali treatment, then taken out and dried at 90°C for 7h.
再把碱处理后的涤纶织物浸渍在上述CA阻燃涂层液中，匀速提拉5min，以均匀涂覆上CA阻燃涂层液。取出涂覆后的涤纶织物，80℃干燥4h。Then, the alkali-treated polyester fabric was dipped in the above-mentioned CA flame retardant coating solution, and pulled at a constant speed for 5 minutes to evenly coat the CA flame retardant coating solution. The coated polyester fabric was taken out and dried at 80°C for 4h.
将干燥后的涤纶织物再浸渍1次CA阻燃涂层液，干燥后制备得到CA涂层阻燃涤纶织物CAP2。The dried polyester fabric was dipped in the CA flame retardant coating solution once again, and the CA coated flame retardant polyester fabric CAP2 was prepared after drying.
实施例3。Example 3.
取2g CMSs-APP阻燃剂，加入到50mL无水乙醇中，40℃下超声处理60min，得到CMSs-APP阻燃剂分散液。Take 2 g of CMSs-APP flame retardant, add it to 50 mL of anhydrous ethanol, and ultrasonically treat it at 40°C for 60 min to obtain a CMSs-APP flame retardant dispersion.
向加有100mL无水乙醇的三颈烧瓶中缓慢加入1g DOPO、4g PVFA，室温下搅拌50min后，再将上述CMSs-APP阻燃剂分散液全部倒入三颈烧瓶中，加热至80℃反应40min，制备得到CA阻燃涂层液。Slowly add 1 g DOPO and 4 g PVFA to a three-necked flask with 100 mL of absolute ethanol, stir at room temperature for 50 min, then pour all the above-mentioned CMSs-APP flame retardant dispersion into the three-necked flask, and heat to 80 °C for reaction 40min, the CA flame retardant coating solution was prepared.
将涤纶织物浸渍于2g/L的NaOH溶液中碱处理40min后，取出，100℃下干燥5h。The polyester fabric was immersed in a 2g/L NaOH solution for 40min alkali treatment, then taken out and dried at 100°C for 5h.
再把碱处理后的涤纶织物浸渍在上述CA阻燃涂层液中，匀速提拉15min，以均匀涂覆上CA阻燃涂层液。取出涂覆后的涤纶织物，100℃干燥2h。Then, the alkali-treated polyester fabric was dipped in the above-mentioned CA flame retardant coating solution, and pulled at a constant speed for 15 minutes to evenly coat the CA flame retardant coating solution. The coated polyester fabric was taken out and dried at 100°C for 2h.
将干燥后的涤纶织物再重复浸渍上述CA阻燃涂层液2次，干燥后制备得到CA涂层阻燃涤纶织物CAP3。The dried polyester fabric was repeatedly dipped in the above CA flame retardant coating solution twice, and after drying, the CA coated flame retardant polyester fabric CAP3 was prepared.
本发明采用扫描电镜(SEM)对涤纶织物上涂覆CA阻燃涂层的形貌进行表征。图1给出了不同处理后涤纶织物的SEM图，其中a～e分别为：纯涤纶织物(Untreated)、碱处理涤纶织物、分别以CA阻燃涂层液浸渍1次的涤纶织物(CAP1)、浸渍2次的涤纶织物(CAP2)和浸渍3次的涤纶织物(CAP3)。从图1中可以清晰看出，纯涤纶织物的纤维拥有光滑且平整的表面；碱处理后的涤纶织物表面明显变得粗糙；浸渍1次阻燃涂层液的织物表面粘附有大量CA颗粒，其平均粒径约为10μm；而随着涂覆次数的增加，织物表面会沉积更多的阻燃涂层，连织物缝隙中也填充了阻燃涂层，浸渍3次阻燃涂层液的织物表面已难以分辨纤维的形貌，阻燃涂层将织物表面完全覆盖。The invention adopts scanning electron microscope (SEM) to characterize the morphology of the CA flame retardant coating on polyester fabric. Figure 1 shows the SEM images of polyester fabrics after different treatments, in which a～e are: pure polyester fabric (Untreated), alkali treated polyester fabric, polyester fabric dipped with CA flame retardant coating solution for one time (CAP1) , polyester fabric impregnated twice (CAP2) and polyester fabric impregnated three times (CAP3). It can be clearly seen from Figure 1 that the fibers of the pure polyester fabric have a smooth and flat surface; the surface of the polyester fabric after alkali treatment becomes obviously rough; the surface of the fabric dipped in the flame retardant coating solution once adheres to a large number of CA particles , and its average particle size is about 10 μm; with the increase of coating times, more flame retardant coatings will be deposited on the surface of the fabric, and even the gaps of the fabric are filled with flame retardant coatings, and the flame retardant coating liquid is dipped three times. The surface of the fabric is difficult to distinguish the morphology of the fiber, and the flame retardant coating completely covers the surface of the fabric.
比较例1。Comparative Example 1.
取2g CMSs-APP阻燃剂，加入到150mL无水乙醇中，40℃超声处理60min，再升温至80℃加热处理40min，得到CMSs-APP阻燃剂分散液。Take 2 g of CMSs-APP flame retardant, add it to 150 mL of anhydrous ethanol, ultrasonically treat it at 40 °C for 60 min, and then heat it up to 80 °C for 40 min to obtain a CMSs-APP flame retardant dispersion.
将涤纶织物浸渍于2g/L的NaOH溶液中碱处理40min后，取出，100℃下干燥5h。The polyester fabric was immersed in a 2g/L NaOH solution for 40min alkali treatment, then taken out and dried at 100°C for 5h.
再把碱处理后的涤纶织物浸渍在上述CA阻燃涂层液中，匀速提拉15min，以均匀涂覆上CA阻燃涂层液。取出涂覆后的涤纶织物，100℃干燥2h。Then, the alkali-treated polyester fabric was dipped in the above-mentioned CA flame retardant coating solution, and pulled at a constant speed for 15 minutes to evenly coat the CA flame retardant coating solution. The coated polyester fabric was taken out and dried at 100°C for 2h.
将干燥后的涤纶织物再重复浸渍上述CA阻燃涂层液2次，干燥后制备得到CA涂层阻燃涤纶织物CAP4。The dried polyester fabric was dipped in the above CA flame retardant coating solution twice again, and the CA coated flame retardant polyester fabric CAP4 was prepared after drying.
本发明针对浸渍不同次数CA阻燃涂层液的涤纶织物进行了LOI和垂直燃烧测试，具体数值展示在表1中。In the present invention, LOI and vertical burning tests are carried out on polyester fabrics dipped in different times of CA flame retardant coating liquid, and the specific values are shown in Table 1.
从表1测试结果可以看出，纯涤纶织物有着极低的极限氧值，且最终消耗殆尽。随着涤纶织物浸渍阻燃涂层液次数的增加，织物的LOI值也随之增加，续燃时间、阴燃时间和损毁长度也有明显下降，且燃烧过程中不会有熔滴滴落，当火焰撤离后出现明显的自熄现象。当浸渍次数为2次及以上时，CAP2、CAP3的LOI值相比纯涤纶织物分别提高了33.8%和37.1%，且均通过了垂直燃烧测试，达到了B1级别。It can be seen from the test results in Table 1 that the pure polyester fabric has a very low limit oxygen value and is eventually exhausted. With the increase of the number of times the polyester fabric is dipped in the flame retardant coating solution, the LOI value of the fabric also increases, and the afterburning time, smoldering time and damage length also decrease significantly, and there will be no dripping during the burning process. Obvious self-extinguishing phenomenon appeared after the flame was withdrawn. When the number of impregnations was 2 or more, the LOI values of CAP2 and CAP3 were increased by 33.8% and 37.1% respectively compared with pure polyester fabrics, and both passed the vertical burning test and reached the B1 level.
而当涂层液中没有添加混合粘结剂时，织物CAP4的LOI值与纯涤纶织物几乎没有变化，且垂直燃烧测试结果也与纯涤纶织物一致，以没有添加混合粘结剂的涂层液处理后的涤纶织物没有阻燃性，说明阻燃剂本身不具有粘附性，不能粘附在涤纶织物的表面。When no mixed binder was added to the coating solution, the LOI value of the fabric CAP4 was almost unchanged from that of the pure polyester fabric, and the vertical burning test results were also consistent with the pure polyester fabric. The treated polyester fabric has no flame retardancy, indicating that the flame retardant itself has no adhesion and cannot adhere to the surface of the polyester fabric.
为进一步分析阻燃涂层对涤纶织物的燃烧影响，本发明分别对纯涤纶织物和不同处理后涤纶织物进行了锥形量热测试。图2展示了不同织物的释热速率曲线HRR(a)和总热释放曲线THR(b)。In order to further analyze the effect of flame retardant coating on the combustion of polyester fabrics, the present invention conducts cone calorimetry tests on pure polyester fabrics and polyester fabrics after different treatments respectively. Figure 2 shows the heat release rate curve HRR(a) and total heat release curve THR(b) of different fabrics.
纯涤纶织物的HRR曲线中产生了一个极强的峰值，是由于PET末端链断裂形成较小的链段，裂解生成挥发性产物导致的结果。而以CA阻燃涂层液涂覆处理后的涤纶织物展示的HRR曲线峰值明显低于纯涤纶织物，且随着涂层次数增加，峰值逐渐减小，其中CAP2和CAP3的HRR相比纯涤纶织物分别降低了51.0%和79.1%。证明阻燃涂层会促使涤纶织物炭化，在织物表面形成一层致密的保护屏障，阻碍了氧气与热量的传递，从而使得HRR和THR有明显的降低。A very strong peak was generated in the HRR curve of pure polyester fabric, which was caused by the fragmentation of the PET terminal chain to form smaller chain segments, which were cracked to generate volatile products. However, the peak value of HRR curve displayed by polyester fabric coated with CA flame retardant coating solution is significantly lower than that of pure polyester fabric, and with the increase of coating times, the peak value gradually decreases. The HRR of CAP2 and CAP3 are compared with pure polyester Fabrics decreased by 51.0% and 79.1%, respectively. It is proved that the flame retardant coating can promote the carbonization of polyester fabrics and form a dense protective barrier on the surface of the fabrics, which hinders the transfer of oxygen and heat, thereby significantly reducing HRR and THR.
进而，为分析阻燃涂层对涤纶织物力学性能的影响，本发明分别对纯涤纶织物和不同处理后涤纶织物进行了拉伸强度测试。图3给出了织物的经向(Warp)和纬向(Weft)拉伸强度测试结果。Furthermore, in order to analyze the influence of the flame retardant coating on the mechanical properties of the polyester fabric, the present invention separately tests the tensile strength of the pure polyester fabric and the polyester fabric after different treatments. Figure 3 presents the results of tensile strength tests in the warp (Warp) and weft (Weft) directions of the fabric.
纯涤纶织物的Warp和Weft拉伸强度分别为28.14MPa和8.93MPa；随着阻燃涂层数增加，涤纶织物的拉伸强度也随之增加，相比纯涤纶织物的Warp和Weft拉伸强度，CAP1分别提高了5.2%和27.5%，CAP2分别提高了11.5%和42.9%，CAP3分别提高了18.1%和58.8%。结果表明阻燃涂层数的增加还有利于提高涤纶织物抵抗外力的能力，这一结果与混合粘合剂的粘合性能有关。混合粘合剂被填充在涤纶织物的缝隙中，使得纤维与纤维之间产生了较强的粘合力，从而增强了涤纶织物的拉伸强度。The Warp and Weft tensile strengths of pure polyester fabrics are 28.14MPa and 8.93MPa, respectively; as the number of flame retardant coatings increases, the tensile strength of polyester fabrics also increases, compared with the Warp and Weft tensile strengths of pure polyester fabrics , CAP1 increased by 5.2% and 27.5%, CAP2 increased by 11.5% and 42.9%, and CAP3 increased by 18.1% and 58.8%, respectively. The results show that the increase in the number of flame retardant coatings is also beneficial to improve the ability of polyester fabrics to resist external forces, which is related to the adhesive properties of the hybrid adhesive. The mixed adhesive is filled in the gaps of the polyester fabric, resulting in strong adhesion between the fibers, thereby enhancing the tensile strength of the polyester fabric.
本发明还考察了阻燃剂与涤纶织物的混合方式对织物力学性能的影响。按照CN109181248A方法将阻燃剂与PET材料进行熔融共混，分别得到阻燃剂含量为2%和3%的CA/PET复合材料，测试其与PET材料的拉伸强度，测试结果如图4所示。The invention also investigates the influence of the mixing mode of the flame retardant and the polyester fabric on the mechanical properties of the fabric. According to the method of CN109181248A, the flame retardant and the PET material were melt-blended to obtain CA/PET composite materials with a flame retardant content of 2% and 3%, respectively. The tensile strength of the flame retardant and the PET material was tested. The test results are shown in Figure 4. Show.
可以看出，纯PET材料的拉伸强度为47.56MPa；随着阻燃剂含量的增加，CA/PET复合材料的拉伸强度随之下降，2% CA/PET与3% CA/PET复合材料的拉伸强度相比纯PET分别下降了24.0%和57.2%。说明熔融共混方式对于PET材料的力学性能会造成一定程度的破坏。因此，本发明选择后处理整理方式对涤纶织物进行阻燃处理，得到的阻燃织物不仅具有优异的阻燃性能，而且织物拉伸强度也有所提高。It can be seen that the tensile strength of pure PET material is 47.56MPa; with the increase of flame retardant content, the tensile strength of CA/PET composite material decreases, 2% CA/PET and 3% CA/PET composite material Compared with pure PET, the tensile strength decreased by 24.0% and 57.2%, respectively. It shows that the melt blending method will cause a certain degree of damage to the mechanical properties of PET materials. Therefore, the present invention selects a post-treatment finishing method to perform flame retardant treatment on the polyester fabric, and the obtained flame retardant fabric not only has excellent flame retardant properties, but also has improved tensile strength of the fabric.
为表征涤纶织物的耐水洗性能，本发明分别将浸渍不同次数阻燃涂层液的涤纶织物浸渍于5g/L的洗涤液中10min，取出清水冲洗干净，晾干。重复洗涤20次。In order to characterize the washing resistance of polyester fabrics, the polyester fabrics dipped in different times of flame retardant coating solution were dipped in 5g/L washing solution for 10min, rinsed with clean water, and air-dried. Repeat washing 20 times.
对水洗后织物进行LOI和垂直燃烧测试，结果列于表2中。可以看出，涤纶织物在水洗20次后，仍然保持着较高的阻燃性能，CAP2水洗后的LOI值为27.7，仍然达到了难燃级别，表明本发明阻燃涂层液具有较好的粘附性和耐水性，在实际应用中可以延长阻燃织物的使用期限。LOI and vertical burn tests were performed on the washed fabrics and the results are listed in Table 2. It can be seen that the polyester fabric still maintains a high flame retardant performance after being washed for 20 times, and the LOI value of CAP2 after washing is 27.7, which still reaches the flame retardant level, indicating that the flame retardant coating solution of the present invention has better flame retardant properties. Adhesion and water resistance, which can extend the service life of flame retardant fabrics in practical applications.
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